CN106589731A - Method for preparing IPN structure PMMA-PU high-transparency composite board through ultrasonic assistance - Google Patents
Method for preparing IPN structure PMMA-PU high-transparency composite board through ultrasonic assistance Download PDFInfo
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- CN106589731A CN106589731A CN201611003998.6A CN201611003998A CN106589731A CN 106589731 A CN106589731 A CN 106589731A CN 201611003998 A CN201611003998 A CN 201611003998A CN 106589731 A CN106589731 A CN 106589731A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
- C08L33/12—Homopolymers or copolymers of methyl methacrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/04—Polymer mixtures characterised by other features containing interpenetrating networks
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a method for preparing an IPN structure PMMA-PU high-transparency composite board through ultrasonic assistance, and belongs to the field of composites. The method comprises the following steps that 1, raw materials (monomers, an initiator/catalyst, a cross-linking agent, a chain extender and the like) of polymethyl methacrylate (PMMA) and polyurethane (PU) are mechanically mixed to be uniform, and the materials are poured into a polytetrafluoroethylene mold after being subjected to vacuum degassing; 2, a sealing pressing head is placed on the mold to apply constant pressure; 3, the mold is placed in a temperature-adjustable low-frequency ultrasonic container, a sequential polymerization reaction is carried out under the action of ultrasonic waves, and the high-transparency interpenetrating polymer network (IPN) structure PMMA-PU composite board is prepared. The action of ultrasonic assistance is adopted, and the prepared IPN structure PMMA-PU composite board has the advantages of being low in microphase separation degree, high in transparency and the like and is expected to be applied to light bulletproof transparent materials.
Description
Technical field
The present invention relates to a kind of preparation method of IPN structures PMMA-PU transparent composite sheet, especially acts in ultrasonic wave added
The preparation method of lower PMMA-PU high grade of transparency composite plates, belongs to field of compound material.
Background technology
Interpenetrating networks（IPN）Structural polymer is two or more polymer blend, different polymer network phases
Mutually run through, and the network structure composite that at least one polymer molecular chain is cross-linked to form in chemical bond mode.IPN structures are answered
Condensation material can by the polymer of the two of different physicochemical properties kinds and the above by interlaced network in macro-scale
Upper composition one is uniform overall, can realize optimal combination at aspects such as mechanics, electricity, calorifics, optical properties, extensively should
For in fields such as engineering plastics, coating, biomedical material, damping materials（CN200780010113.8,
CN200480018292.6, CN201510056145.8, CN200710100042.2）.
The existing numerous studies work of IPN architectural polymeric materials at present, but majority concentrates on engineering plastics field, for saturating
The research of bright material is little.According to component polymer polymerization time order difference, IPN structural polymers are divided into simultaneous polymerization and suitable
Sequence two classes of polymerization, difference of them is component polymer polymerization time order, and the former is the polyreaction of different component polymer
Carry out simultaneously, and the latter to be a kind of polyreaction of component carried out first, pre-polymerization to a certain extent when by rising a high reaction temperature,
Cause the polyreaction of other components, form the polymer network for mutually running through.Jehl etc. have studied IPN structures PMMA-PU and gather
The transparency of compound, because chain extender polypropylene glycol PPG and PMMA have different refractivity, will have residue to deposit when PPG is excessive
Polymer devitrification, any method that can improve biphase dispersibility is being caused all to be conducive to transparency（The transparency of polyurethane-poly(methyl methacrylate) interpenetrating and semi-interpenetrating polymer networks[J], European Polymer Journal, 1983; 19 (7): 597-600）.Due to refractive index mismatch and split-phase is serious between different polymer raw material component in simultaneous polymerization method, cause
Transparency is low, therefore, generally transparent interpenetrating net polymer is prepared using sequential polymerization（Simultaneous interpenetrating networks of a polyurethane and poly(methyl methacrylate). 1.Metastable phase diagrams[J], Journal of Applied Polymer Science, 1995; 58 (2): 331-346）.
Fang etc. mixes PMMA using seed emulsion polymerization in aqueouss PU, prepares with core-shell structure copolymer pattern, nano junction
The polyphasic PU-PMMA composites of structure（Tailoring elastomeric properties of waterborne polyurethane by incorporation of polymethyl methacrylate with nanostructural heterogeneity[J], RSC Advance, 2016; 6: 13589-13599）, realize PU elasticity modulus of materials, stretching
Intensity, elongation after fracture, heat stability and resistance to water controllable adjustment, but its light transmission is relatively low.Heim etc. adopts simultaneous polymerization
Method prepares a small amount of PU of addition（Less than 10%）The PMMA casting plates of reinforcing, the variation tendency phase of sheet material transparency and impact property
Instead, but all relevant with PMMA node sizes, the crosslink density of swelling PU networks, works as PMMA when the latter starts to be polymerized depending on MMA
Sheet material light transmission is poor when node size is more than 1 micron（High impact cast sheets of poly(methyl methacrylate) with low levels of polyurethane[J], Polymer, 1993; 34(8): 1653- 1660）.
Kim etc. have studied ambient pressure for simultaneous polymerization method prepares the shadow of IPN structure PMMA-PU composite patterns
Ring, with pressure rise, the regional scale of PU phases is reduced to 3 nm by 30 nm, and PU is improved with the PMMA compatibilitys, composite by
Under normal pressure it is opaque be changed into it is transparent（Polyurethane interpenetrating polymer networks synthesized under high pressure. 1. [J], Macromolecules, 1984; 17: 268-272）.
The physical property of IPN structure PMMA-PU polymer prepared by the comparative studies such as Bird simultaneous polymerization method and sequential polymerization, together
The transparency of step polymerization is 40-70%, and sequential polymerization is due to phase separation low degree（Dispersion is high）, transparency reaches 70-
90%（Synthesis and characterization of high performance, transparent interpenetrating polymer networks with polyurethane and poly(methyl methacrylate)[J], Polymer Engineering and Science, 2013; 53(4): 716-723）.
Berrebi etc. is prepared for the fatty poly-ester carbonate PC/PMMA polymer of IPN structures using simultaneous polymerization method, and its transparency is high
Up to 95%, this refractive index close with two kinds of phases（n= 1.498(PC), 1.491 (PMMA)）And phase separation low degree is relevant
（Development of organic glass using interpenetrating polymer networks with enhanced resistance towards scratches and solvents[J], European Polymer Journal, 2015; 63: 132- 140）.
The content of the invention
It is an object of the invention to provide a kind of preparation side of ultrasonic wave added IPN structures PMMA-PU high grade of transparency composite plate
Method, compared with Traditional IP N structure PMMA-PU composite, the present invention is on the basis of pressurization sequence polymerization, to be shaken by ultrasound
Assosting effect is swung, the area size of PMMA and PU phases is reduced, dispersibility and the compatibility of two kinds of phases is improved, it is multiple so as to be obviously improved
The light transmission of plywood, prepares high grade of transparency IPN structure PMMA-PU composite.
The object of the present invention is achieved like this, a kind of system of ultrasonic wave added IPN structures PMMA-PU high grade of transparency composite plate
Preparation Method, it is characterised in that realized by following processing step：
1）By quantitative aliphatic isocyanates, polyether polyol, chain extender and catalytic mechanical mix homogeneously, polyurethane is configured
（PU）Material solution；
2）By quantitative methyl methacrylate（MMA）, initiator and cross-linking agent mechanical mixture it is uniform, configure polymethylacrylic acid
Methyl ester（PMMA）Material solution；
3）By the material solution mix homogeneously of PMMA and PU, vacuum outgass, in pouring Teflon mould into, by the upper of mould
Pressure head is sealed to mixed solution, and applies constant pressure, and the pre-polymerization of mixed solution is carried out at a certain temperature；
4）Mould is immersed in homoiothermic low frequency ultrasound container in water, the sequential polymerization heated up using echelon, with reference to a constant temperature
Sonic oscillation under degree, prepares the PMMA-PU transparent composite sheets of IPN structures.
Described PMMA and the mass ratio of PU is 4.
Described aliphatic isocyanates are isophorone diisocyanate（IPDI）, polyether polyol is polypropylene glycol
（PPG）, molecular weight is 900～1100；Isocyanate index（K=NCO/OH）For 1.1；Chain extender is 1,4-butanediol（BDO）,
Its usage amount is the 10～20% of PPG mass；Catalyst is dibutyl tin laurate（DBTDL）, its usage amount is PPG and BDO
The 1% of quality summation.
Described initiator is azodiisobutyronitrile（AIBN）, its usage amount is the 0.2%～1.0% of MMA mass；Cross-linking agent
For trimethylol-propane trimethacrylate（TMPTMA）, its usage amount is the 2%～8% of MMA mass.
Described constant pressure is 100～200 MPa；50 degrees Celsius of the pre-polymerization temperature of mixed solution, pre-polymerization time 0.5
～2 h.
The sequential polymerization technique that described echelon heats up is 60 degrees Celsius of h of constant temperature 5, is warming up to 70 degrees Celsius of h of constant temperature 5,
80 degrees Celsius of h of constant temperature 5 are warming up to, 95 degrees Celsius of h of constant temperature 2 are warming up to.
Described sonic oscillation frequency is 20～40 kHz, and ultrasonic power is 30～60 W, and the temperature of sonic oscillation is 60
Degree Celsius.
The Teflon mould is made up of square container and seaming chuck, and square container is homoiothermic low frequency ultrasound container,
Water is installed in homoiothermic low frequency ultrasound container, support is provided with its bottom, sealed mold is installed on support, sealed mold is built-in with
Seaming chuck and composite plate, support bottom is provided with sonic oscillation instrument.Mould is immersed in homoiothermic low frequency ultrasound container in experimentation
In interior water, and apply constant pressure P in seaming chuck.
Compared with existing IPN structures PMMA-PU composite material and preparation method thereof, there is the present invention substantial advance and technology to create
Newly, it is embodied in：
1）The mechanical effect of sonic oscillation can improve the mixing uniformity of PU performed polymers and MMA monomer solutions, in polyreaction
During, by sonic oscillation shear action, reduce PU and PMMA molecular chain lengths, improves the degree that run through between strand；
Molecule diffusional resistance increase under external pressure effect, Inhibitory molecules chain movement, so as to significantly reduce the microfacies of single polymers
Size and microphase separation degree, obtain high grade of transparency IPN composite sheet structure；
2）The cavitation effect of sonic oscillation advantageously reduces PU performed polymers and the bubble cuclear density in MMA monomer solutions, reduces multiple
Gas hole defect in plywood；The heat effect and chemical effect of sonic oscillation can accelerate the step-by-step polymerization reaction of PU and the freedom of PMMA
Base polyreaction.
In sum, the present invention is acted on using ultrasonic wave added, is conducive to being substantially reduced out of phase during sequential polymerization
Area size, the biphase dispersibility of raising and the compatibility, prepare high grade of transparency IPN structure PMMA-PU composite plate.
Description of the drawings
The experimental provision schematic diagram of the present invention of accompanying drawing 1, Teflon mould is made up of square container and seaming chuck in figure, real
Mould is immersed in homoiothermic low frequency ultrasound container in water during testing, and applies constant pressure P in seaming chuck.
Accompanying drawing 2 is ultrasonic wave added IPN structure PMMA-PU transparent composite sheets of the invention.
In figure, 1, homoiothermic low frequency ultrasound container, 2, seaming chuck, 3, water, 4, support, 5, sealed mold, 6, composite plate, 7,
Sonic oscillation instrument.
Specific embodiment
Embodiment 1
The PMMA monomer solutions of 100 g are prepared, 94.5 g MMA monomers are taken, adds 5.0 g cross-linking agent TMPTMA and 0.5 g to draw
Agent AIBN, the min of mechanical agitation 5 are sent out, it is standby.
The PU monomer solutions of 100 g are prepared, 34.8 g isophorone diisocyanate IPDI are taken, 56.8 g poly- third are added
Glycol PPG, 7.7 g chain extenders BDO and 0.7 g catalyst DBTDL, the min of mechanical agitation 5, it is standby.
Sample is roughly ground and fine grinding using 250 mesh and 2000 mesh emery papers respectively, and using liquid paraffin and surpassed
Fine silica powder body prepares abrasive pastes, is processed by shot blasting on flannelette surface, obtains thickness and is about the transparent compound of 3.5 mm
Plate, as shown in Figure 2.Using the optical property of photoelectricity haze meter test compound plate, its transparency is 91.6%.
Embodiment 2
Uniform, the vacuum outgass by PMMA the and PU monomer solutions mechanical mixture in example 1, in pouring Teflon mould into, lead to
The seaming chuck for crossing mould is sealed to mixed solution, applies constant pressure P=120 MPa, 50 degrees Celsius of h of lower pre-polymerization 2.Will
Mould is immersed in homoiothermic low frequency ultrasound container in water, and water temperature is 60 degrees Celsius, and the h of constant temperature 5 is warming up to 70 degrees Celsius of constant temperature 5
H, is warming up to 80 degrees Celsius of h of constant temperature 5, is warming up to 95 degrees Celsius of h of constant temperature 2, and the PMMA-PU for preparing IPN structures is transparent multiple
Plywood.
Sample is roughly ground and fine grinding using 250 mesh and 2000 mesh emery papers respectively, and using liquid paraffin and surpassed
Fine silica powder body prepares abrasive pastes, is processed by shot blasting on flannelette surface, obtains thickness and is about the transparent compound of 3.4 mm
Plate.Using the optical property of photoelectricity haze meter test compound plate, its transparency is 88.2%.
As shown in Figure 1-2, the Teflon mould is made up of square container and upper pressure/2, and square container is that homoiothermic is low
The ultrasonic container 1 of frequency, installs water 3 in homoiothermic low frequency ultrasound container 1, support 4 is provided with its bottom, and sealed mold is installed on support
5, sealed mold 5 is built-in with seaming chuck 2 and composite plate 6, and support bottom is provided with sonic oscillation instrument 7.Mould leaching in experimentation
Not in water 3 in homoiothermic low frequency ultrasound container 1, and apply constant pressure P in seaming chuck.
Claims (7)
1. a kind of preparation method of ultrasonic wave added IPN structures PMMA-PU high grade of transparency composite plate, its feature includes following technique step
Suddenly：
1）By quantitative aliphatic isocyanates, polyether polyol, chain extender and catalytic mechanical mix homogeneously, polyurethane is configured
（PU）Material solution；
2）By quantitative methyl methacrylate（MMA）, initiator and cross-linking agent mechanical mixture it is uniform, configure polymethylacrylic acid
Methyl ester（PMMA）Material solution；
3）By the material solution mix homogeneously of PMMA and PU, vacuum outgass, in pouring Teflon mould into, by the upper of mould
Pressure head is sealed to mixed solution, and applies constant pressure, and the pre-polymerization of mixed solution is carried out at a certain temperature；
4）Mould is immersed in homoiothermic low frequency ultrasound container in water, the sequential polymerization technique heated up using echelon, with reference to certain
At a temperature of sonic oscillation, prepare the PMMA- PU transparent composite sheets of IPN structures.
2. the preparation method of a kind of ultrasonic wave added IPN structures PMMA-PU high grade of transparency composite plate according to claim 1,
It is characterized in that：The mass ratio of PMMA and PU is 4.
3. the preparation method of a kind of ultrasonic wave added IPN structures PMMA-PU high grade of transparency composite plate according to claim 1,
It is characterized in that：Described aliphatic isocyanates are isophorone diisocyanate（IPDI）, polyether polyol is poly- the third two
Alcohol（PPG）, molecular weight is 900～1100；Isocyanate index（K=NCO/OH）For 1.1；Chain extender is 1,4-butanediol
（BDO）, its usage amount is the 10～20% of PPG mass；Catalyst is dibutyl tin laurate（DBTDL）, its usage amount is
The 1% of PPG and BDO mass summations.
4. the preparation method of a kind of ultrasonic wave added IPN structures PMMA-PU high grade of transparency composite plate according to claim 1,
It is characterized in that：Described initiator is azodiisobutyronitrile（AIBN）, its usage amount is the 0.2%～1.0% of MMA mass；Hand over
Connection agent is trimethylol-propane trimethacrylate（TMPTMA）, its usage amount is the 2%～8% of MMA mass.
5. the preparation method of a kind of ultrasonic wave added IPN structures PMMA-PU high grade of transparency composite plate according to claim 1,
It is characterized in that：Described constant pressure is 100～200 MPa；The pre-polymerization temperature of mixed solution is 50 degrees Celsius, during pre-polymerization
Between 0.5～2 h.
6. the preparation method of a kind of ultrasonic wave added IPN structures PMMA-PU high grade of transparency composite plate according to claim 1,
It is characterized in that：The sequential polymerization technique that described echelon heats up is 60 degrees Celsius of h of constant temperature 5, is warming up to 70 degrees Celsius of constant temperature 5
H, is warming up to 80 degrees Celsius of h of constant temperature 5, is warming up to 95 degrees Celsius of h of constant temperature 2.
7. the preparation method of a kind of ultrasonic wave added IPN structures PMMA-PU high grade of transparency composite plate according to claim 1,
It is characterized in that：Described sonic oscillation frequency is 20～40 kHz, and ultrasonic power is 30～60 W, and the temperature of sonic oscillation is
60 degrees Celsius.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107083002A (en) * | 2017-04-27 | 2017-08-22 | 蚌埠承永玻璃制品有限公司 | A kind of heat-resistant high-strength lucite and preparation method thereof |
| CN110511657A (en) * | 2019-08-08 | 2019-11-29 | 上海航天化工应用研究所 | A kind of solar heat protection binding function integrated composite of low-temperature curable and its preparation method and application |
| CN113580415A (en) * | 2021-08-02 | 2021-11-02 | 浙江省林业科学研究院 | Solution suspension device and method for preparing bamboo fiber glass fiber net prefabricated body |
Citations (1)
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| CN105622857A (en) * | 2016-04-01 | 2016-06-01 | 武汉大学 | Preparation method of interpenetrating-network-structure water-based polyurethane nano composite material |
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2016
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105622857A (en) * | 2016-04-01 | 2016-06-01 | 武汉大学 | Preparation method of interpenetrating-network-structure water-based polyurethane nano composite material |
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| S. C . KIRN,ETAL: "Polyurethane Interpenetrating Polymer Networks.I. Synthesis and Morphology of Polyurethane-Poly (methyl methacrylate) Interpenetrating Polymer Networks", 《MACROMOLECULES》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107083002A (en) * | 2017-04-27 | 2017-08-22 | 蚌埠承永玻璃制品有限公司 | A kind of heat-resistant high-strength lucite and preparation method thereof |
| CN110511657A (en) * | 2019-08-08 | 2019-11-29 | 上海航天化工应用研究所 | A kind of solar heat protection binding function integrated composite of low-temperature curable and its preparation method and application |
| CN110511657B (en) * | 2019-08-08 | 2021-06-11 | 上海航天化工应用研究所 | Low-temperature-curable heat-proof bonding function integrated composite material and preparation method and application thereof |
| CN113580415A (en) * | 2021-08-02 | 2021-11-02 | 浙江省林业科学研究院 | Solution suspension device and method for preparing bamboo fiber glass fiber net prefabricated body |
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